CN105001270A - Preparing method for Ba/Fe/Na metal and carboxylic acid Schiff base complex - Google Patents
Preparing method for Ba/Fe/Na metal and carboxylic acid Schiff base complex Download PDFInfo
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Abstract
The invention belongs to the technical field of chemistry and particularly relates to a preparing method and application based on a Ba/Fe/Na metal and carboxylic acid Schiff base complex. The chemical formula of the complex is (BaNa(Fe-L)2(Mu2-OH)(H2O)).DMF.2H2O, wherein L is a 1, 2-cyclohexane diamino-N, N'-di(3-methyl-5-carboxyl salicylaldehyde) negative ion from which four protons are removed. The complex is prepared by adopting a solvent-thermal method. Researches on organic pollutant light catalytic degradation of the complex show that the complex can degrade 2-monochlorphenol, 3-monochlorphenol and 4-monochlorphenol under irradiation of visible light, has the best light degradation efficacy on 4-monochlorphenol, and is expected to be applied to the field of material science as a catalyst for organic pollutant light degradation.
Description
Technical field
The invention belongs to technical field of chemistry, be specifically related to a kind of transition metal complex preparation method and application thereof.
Background technology
Assorted metal-organic framework due to have in magnetic, gas adsorption and heterocatalysis etc. potential application and by chemist extensive concern (T. Senapati, C. Pichon, R. Ababei, C. Mathonie re, R. Cle rac,
inorg. Chem. 2012,51,3796).Functionalized Schiff's base is the splendid part of the assorted metal complexes of preparation, reason be the cavity of Schiff's base inside and outside functional group can from different metals coordination (K. Bhattacharya, S. M. T. Abtab respectively, M. C. Majee, A. Endo, M. Chaudhury
inorg. Chem. 2014,53,8287).
Photochemical catalysis is also a current study hotspot, this technology be widely used in gas and water purification with to be separated etc. field (H. Zhang, L.-H. Guo, L. Zhao, B. Wan, Y. Yang,
j. Phys. Chem. Lett. 2015,6,958).Recent research shows, the assorted metal complexes of several iron content has the performance of photodegradation organic pollutant (D. S. Nesterov, E. N. Chygorin, V. N. Kokozay, V. Bon, R. Boca, Y. N. Kozlov, L. S. Shul ' pina, J. Jezierska, A. Ozarowski, A. J. L. Pombeiro, G. B. Shul ' pin
inorg. Chem. 2012,51,9110).But the three assorted metal complexess based on carboxylic acid functional schiff base ligand are also unmanned so far to be reported.
Summary of the invention
The technical problem to be solved in the present invention is open a kind of assorted metal complexes based on Ba/Fe/Na tri-kinds of metals and carboxylic acid schiff base ligand.
The present invention also discloses preparation method and the application thereof of this assorted metal complexes.
Assorted metal complexes has following chemical formula, that is: [BaNa (Fe-L)
2(
μ 2 -OH) (H
2o)] DMF2H
2o, wherein L is 1,2-hexanaphthene diamino-N of four protons, N'-bis-(3-methyl-5-carboxylsalicylidene) anion ligand.
Complex crystal belongs to rhombic system, and spacer is
f222, unit cell parameters is
a=31.955 (3),
b=65.386 (2),
c=12.9570 (16),
α=90 °,
β=90 °,
γ=90 °,
v=27072 (4)
3, basic structure is the three-dimensional frame structure containing duct.
The preparation method of described assorted metal complexes, comprises the steps:
Get BaCl
22H
2o 0.12 mmol, 1,2-hexanaphthene diamino-N, N'-bis-(3-methyl-5-carboxylsalicylidene) (H
4l part) 0.03 mmol, FeCl
36H
2o 0.03 mmol, NaCl 0.06 mmol, dimethyl formamide 1 mL, ethanol 4 mL and water 2 mL mix, and obtain brown suspension.Mixture is put into 15 mL tetrafluoroethylene reactors, place in an oven, be heated to 100 DEG C of constant temperature 72 hours, then slowly drop to room temperature and obtain brown crystal, productive rate 31%.
Crystal prototype of the present invention is to the 2-chlorophenol under radiation of visible light, and 3-chlorophenol and 4-chlorophenol all show photocatalytic degradation capability, wherein the strongest to the photocatalytic degradation capability of 4-chlorophenol, can be applied as Photodegradation catalyst at material science.
The present invention's metal complexes of mixing is obtained by solvent-thermal process, has the features such as preparation method is simple, product performance stable, repeatability is strong.
Accompanying drawing explanation
Fig. 1 is the coordination environment figure of metal in title complex;
Fig. 2 is three-dimensional open-framework figure;
When Fig. 3 is different pH value, title complex photocatalytic degradation 2-chlorophenol time history plot;
When Fig. 4 is different pH value, title complex photocatalytic degradation 3-chlorophenol time history plot;
When Fig. 5 is different pH value, title complex photocatalytic degradation 4-chlorophenol time history plot;
Fig. 6 is the powder diagram of title complex.
Embodiment
The synthesis of assorted metal complexes:
Embodiment 1
Get barium chloride dihydrate 0.12 mmol, ferric chloride hexahydrate 0.03 mmol, sodium-chlor 0.06 mmol and H
4l part 0.03 mmol, puts into 15 mL tetrafluoroethylene reactors, with 1 mL dimethyl formamide, 4 mL ethanol and 2 mL water are mixed solvent, place in an oven, are heated to 100 DEG C of constant temperature 72 hours, then slowly drop to room temperature and obtain brown crystal, productive rate 31%.
Embodiment 2
Get barium chloride dihydrate 0.12 mmol, ferric chloride hexahydrate 0.03 mmol, sodium-chlor 0.06 mmol and H
4l part 0.03 mmol, puts into 15 mL tetrafluoroethylene reactors, with 3 mL dimethyl formamides, 2 mL ethanol and 2 mL water are mixed solvent, place in an oven, are heated to 110 DEG C of constant temperature 72 hours, then slowly drop to room temperature and obtain brown crystal, productive rate 10%.
Main infrared absorption peak is: 3394 (m), 2932 (w), 2858 (w), 1607 (w), 1565 (w), 1388 (w), 1308 (w), 1286 (w), 1217 (w), 1122 (m), 1027 (s), 978 (s), 952 (s), 919 (s), 861 (s), 794 (m), 760 (m), 712 (m), 582 (m), 558 (m), 525 (m), 502 (s), 466 (m), 421 (s).
The relevant characterization of title complex
(1) crystal structure determination of title complex
The diffraction data of title complex collects on Oxford Diffraction Gemini R Ultra diffractometer, 293 K, Mo K
αray (λ=0.71069).Operation technique scanning corrects.Crystalline structure is solved with direct method by SHELEXL-97 program, carries out refine with complete matrix method of least squares SHELEXL-97.The temperature factor anisotropy of non-hydrogen atom is revised.Detailed axonometry data are in table 1; Important bond distance and bond angle data are in table 2; Crystalline structure is shown in Fig. 1 and Fig. 2.
The title complex of invention is characterized in that described complex crystal belongs to rhombic system, and spacer is
f222, unit cell parameters is
a=31.955 (3),
b=65.386 (2),
c=12.9570 (16),
α=90 °,
β=90 °,
γ=90 °,
v=27072 (4)
3.Comprise two independently Fe (III) ions (Fe1 and Fe2 is half occupation rate, pentacoordinate configuration) in unit cell, three independently Ba (II) ion (wherein Ba1 and Ba2 is 1/4th occupation rates, eight-coordinate configuration; Ba3 is half occupation rate, hexa-coordinate configuration), two Na (I) ions (Na1 and Na2 is half occupation rate, four-coordination configuration), two each and every one L
4-negatively charged ion, two half occupation rates
μ 2-OH negatively charged ion, the coordinated water molecule of two half occupation rates, a free DMF molecule and two free water moleculess.Two iron ions are embedded in two L respectively
4-the N of negatively charged ion inside
2o
2in, by one
μ 2-OH negatively charged ion connects for (Fe-L)
2(
μ 2-OH) dimer.Two L
4-negatively charged ion respectively with (three Ba ion/two Na ions) and (two Ba ion/two Na ions) coordination.The one-piece construction of title complex is the three-dimensional framework containing duct.
(2) the photochemical catalysis 2-chlorophenol of title complex, 3-chlorophenol and 4-chlorophenol research (30m long × 0.25mm i.d., WondaCAP 17 capillary chromatography, GC-2014C, Shimadzu, FID detector).
Under visible light illumination, title complex all plays obvious Degradation to the concentration of three kinds of chlorophenols in solution.Under the condition of pH=3, be 55.5%(Fig. 3 to the photodegradative ability of 2-chlorophenol); Under the condition of pH=4, be 40.3%(Fig. 4 to the photodegradative ability of 3-chlorophenol); Under the condition of pH=3, be 71%(Fig. 5 to the photodegradative ability of 4-chlorophenol).
(3) the XPRD phase purity of title complex characterizes (Rigaku Dmax 2000 X-ray diffraction device).
Complex crystal is detected and as the phase purity after catalyzer by powder x-ray diffraction.Finding that the position at main PXRD peak is identical by comparing, the integrity maintaining crystallinity and structure being described, seeing Fig. 6 as title complex after catalyzer.
Table 1 is the predominant crystal data of title complex
| formula | C 51H 51N 5O 17Fe 2BaNa |
| Mr | 1277.34 |
| crystal system | orthographic |
| space group | F222 |
| a (?) | 31.955(3) |
| b (?) | 65.386(2) |
| c (?) | 12.9570(16) |
| α(°) | 90 |
| β(°) | 90 |
| γ(°) | 90 |
| V (? 3) | 27072(4) |
| Z | 16 |
| D calc (g cm -3) | 1.116 |
| F(0 0 0) | 9112 |
| R int | 0.0437 |
| GOF on F 2 | 1.026 |
| R1 [I>2σ(I)] | 0.0818 |
| wR2 (all data) | 0.2554 |
Table 2 is main bond distance's () and the bond angle [°] of title complex
*
| Fe(1)-O(2) | 1.7718(19) | Fe(1)-O(8) | 1.908(5) |
| Fe(1)-O(7) | 1.934(6) | Fe(2)-O(1) | 1.7665(14) |
| Fe(2)-O(5) | 1.899(5) | Fe(2)-O(6) | 1.898(5) |
| Fe(1)-N(4) | 2.067(6) | Fe(1)-N(3) | 2.133(6) |
| Fe(2)-N(2) | 2.095(6) | Fe(2)-N(1) | 2.103(5) |
| Ba(1)-O(13) #1 | 2.697(12) | Ba(1)-O(13) #2 | 2.697(12) |
| Ba(1)-O(13) | 2.697(12) | Ba(1)-O(13) #3 | 2.697(12) |
| Ba(1)-O(11) #3 | 2.752(6) | Ba(1)-O(11) #2 | 2.752(6) |
| Ba(1)-O(11) | 2.752(6) | Ba(1)-O(11) #1 | 2.752(6) |
| Ba(2)-O(4) #4 | 2.719(11) | Ba(2)-O(4) #5 | 2.719(11) |
| Ba(2)-O(4) #6 | 2.719(11) | Ba(2)-O(4) #3 | 2.719(11) |
| Ba(2)-O(10) #7 | 2.861(11) | Ba(2)-O(10) #8 | 2.861(11) |
| Ba(2)-O(10) | 2.861(11) | Ba(2)-O(10) #9 | 2.861(11) |
| Ba(3)-O(3) | 2.445(15) | Ba(3)-O(9) #11 | 2.535(11) |
| Ba(3)-O(3) #10 | 2.566(15) | Ba(3)-O(2W) #10 | 2.658(14) |
| Ba(3)-O(9) #12 | 2.816(11) | Ba(3)-O(2W) | 2.860(15) |
| Ba(3)-O(4) | 2.992(11) | Ba(3)-O(4) #10 | 3.039(11) |
| Na(1)-O(14) | 2.678(16) | Na(1)-O(14) #2 | 2.678(16) |
| Na(1)-O(12) #2 | 2.683(10) | Na(1)-O(12) | 2.683(10) |
| Na(2)-O(1W) | 2.477(18) | Na(2)-O(9) #11 | 2.746(10) |
| Na(2)-O(4) | 2.936(11) | Na(2)-O(10) #3 | 2.984(13) |
| O(2)-Fe(1)-O(8) | 117.15(19) | O(2)-Fe(1)-O(8) | 106.3(3) |
| O(8)-Fe(1)-O(7) | 89.9(2) | O(2)-Fe(1)-N(4) | 107.8(2) |
| O(8)-Fe(1)-N(4) | 133.8(2) | O(7)-Fe(1)-N(4) | 87.3(2) |
| O(2)-Fe(1)-N(3) | 85.1(2) | O(7)-Fe(1)-N(3) | 153.7(2) |
| N(4)-Fe(1)-N(3) | 77.8(3) | O(1)-Fe(2)-O(6) | 113.4(2) |
| O(1)-Fe(2)-O(5) | 112.4(3) | O(6)-Fe(2)-O(5) | 89.1(2) |
| O(1)-Fe(2)-N(2) | 100.8(2) | O(6)-Fe(2)-N(2) | 85.5(2) |
| O(5)-Fe(2)-N(2) | 145.6(3) | O(1)-Fe(2)-N(1) | 100.9(2) |
| O(6)-Fe(2)-N(1) | 143.9(2) | O(5)-Fe(2)-N(1) | 87.9(2) |
| N(2)-Fe(2)-N(1) | 77.1(3) | O(13) #1-Ba(1)-O(13) #2 | 110.0(5) |
| O(13) #1-Ba(1)-O(13) | 134.3(5) | O(13) #2-Ba(1)-O(13) | 87.7(5) |
| O(13) #1-Ba(1)-O(13) #3 | 87.7(5) | O(13) #2-Ba(1)-O(13) #3 | 134.3(5) |
| O(13) #1-Ba(1)-O(13) #3 | 110.0(5) | O(13) #1-Ba(1)-O(11) #3 | 73.5(3) |
| O(13) #2-Ba(1)-O(11) #3 | 149.2(3) | O(13)-Ba(1)-O(11) #3 | 71.2(3) |
| O(13) #3-Ba(1)-O(11) #3 | 75.4(3) | O(13) #1-Ba(1)-O(11) #2 | 71.2(3) |
| O(13) #2-Ba(1)-O(11) #2 | 75.4(3) | O(13)-Ba(1)-O(11) #2 | 73.5(3) |
| O(13) #3-Ba(1)-O(11) #2 | 149.2(3) | O(11) #3-Ba(1)-O(11) #2 | 77.1(4) |
| O(13) #1-Ba(1)-O(11) | 149.2(3) | O(13) #2-Ba(1)-O(11) | 73.5(13) |
| O(13)-Ba(1)-O(11) | 75.4(3) | O(13) #3-Ba(1)-O(11) | 71.2(3) |
| O(11) #3-Ba(1)-O(11) | 120.0(4) | O(11) #2-Ba(1)-O(11) | 136.3(4) |
| O(13) #1-Ba(1)-O(11) #1 | 75.4(3) | O(13) #2-Ba(1)-O(11) #1 | 71.2(3) |
| O(13)-Ba(1)-O(11) #1 | 149.2(3) | O(13) #3-Ba(1)-O(11) #1 | 73.5(3) |
| O(11) #3-Ba(1)-O(11) #1 | 136.3(4) | O(11) #2-Ba(1)-O(11) #1 | 120.0(4) |
| O(11)-Ba(1)-O(11) #1 | 77.1(4) | O(4) #4-Ba(2)-O(4) #5 | 99.0(4) |
| O(4) #4-Ba(2)-O(4) #6 | 150.6(4) | O(4) #5-Ba(2)-O(4) #6 | 88.4(4) |
| O(4) #4-Ba(2)-O(4) #3 | 88.4(4) | O(4) #5-Ba(2)-O(4) #3 | 150.6(4) |
| O(4) #6-Ba(2)-O(4) #3 | 99.0(4) | O(4) #4-Ba(2)-O(10) #7 | 72.3(3) |
| O(4) #5-Ba(2)-O(10) #7 | 70.7(3) | O(4) #6-Ba(2)-O(10) #7 | 83.7(3) |
| O(4) #3-Ba(2)-O(10) #7 | 138.1(3) | O(4) #4-Ba(2)-O(10) #8 | 83.7(3) |
| O(4) #5-Ba(2)-O(10) #8 | 138.1(3) | O(4) #6-Ba(2)-O(10) #8 | 72.3(3) |
| O(4) #3-Ba(2)-O(10) #8 | 70.7(3) | O(10) #7-Ba(2)-O(10) #8 | 70.5(5) |
| O(4) #4-Ba(2)-O(10) | 138.1(3) | O(4) #5-Ba(2)-O(10) | 83.7(3) |
| O(4) #6-Ba(2)-O(10) | 70.7(3) | O(4) #3-Ba(2)-O(10) | 72.3(3) |
| O(10) #7-Ba(2)-O(10) | 144.3(5) | O(10) #8-Ba(2)-O(10) | 121.5(4) |
| O(4) #4-Ba(2)-O(10) #9 | 70.7(3) | O(4) #5-Ba(2)-O(10) #9 | 72.3(3) |
| O(4)-Ba(2)-O(10) #9 | 138.1(3) | O(4)-Ba(2)-O(10) #9 | 83.7(3) |
| O(10)-Ba(2)-O(10) #9 | 121.5(4) | O(10)-Ba(2)-O(10) #9 | 144.3(5) |
| O(10)-Ba(2)-O(10) #9 | 70.5(5) | O(3)-Ba(3)-O(9) #11 | 79.4(4) |
| O(3)-Ba(3)-O(3) #10 | 161.8(6) | O(9) #11-Ba(3)-O(3) #10 | 97.1(4) |
| O(3)-Ba(3)-O(2W) #10 | 82.5(4) | O(9) #11-Ba(3)-O(2W) #10 | 91.1(5) |
| O(3) #10-Ba(3)-O(2W) #10 | 115.5(4) | O(3)-Ba(3)-O(9) #12 | 92.9(4) |
| O(9) #11-Ba(3)-O(9) #12 | 115.6(4) | O(3) #10-Ba(3)-O(9) #12 | 72.3(4) |
| O(2W) #10-Ba(3)-O(9) #12 | 151.7(4) | O(3)-Ba(3)-O(2W) | 112.6(4) |
| O(9) #1-Ba(3)-O(2W) | 159.3(4) | O(3) #10-Ba(3)-O(2W) | 76.6(4) |
| O(2W) #10-Ba(3)-O(2W) | 74.6(8) | O(9) #12-Ba(3)-O(2W) | 81.6(4) |
| O(3)-Ba(3)-O(4) | 43.6(4) | O(3)-Ba(3)-O(4) | 65.4(3) |
| O(9) #11-Ba(3)-O(4) | 118.7(4) | O(3) #10-Ba(3)-O(4) | 122.6(4) |
| O(9) #12-Ba(3)-O(4) | 66.1(3) | O(3)-Ba(3)-O(4) | 134.9(3) |
| O(3)-Ba(3)-O(4) #10 | 121.1(4) | O(9) #11-Ba(3)-O(4) #10 | 68.7(3) |
| O(3) #10-Ba(3)-O(4) #10 | 42.6(4) | O(2W) #10-Ba(3)-O(4) #10 | 143.0(3) |
| O(9) #12-Ba(3)-O(4) #10 | 61.8(3) | O(2W)-Ba(3)-O(4) #10 | 114.4(4) |
| O(4)-Ba(3)-O(4) #10 | 77.9(4) | O(14)-Na(1)-O(14) #2 | 138.5(7) |
| O(14)-Na(1)-O(12) #2 | 68.1(4) | O(14) #2-Na(1)-O(12) #2 | 85.0(4) |
| O(14)-Na(1)-O(12) | 85.0(4) | O(14) #2-Na(1)-O(12) | 68.1(4) |
| O(12) #2-Na(1)-O(12) | 99.1(5) | O(1W)-Na(2)-O(9) #11 | 92.9(6) |
| O(1W)-Na(2)-O(4) | 118(1) | O(9) #11-Na(2)-O(4) | 63.9(3) |
| O(1W)-Na(2)-O(10) #3 | 59.5(8) | O(9) #11-Na(2)-O(10) #3 | 97.1(3) |
| O(4)-Na(2)-O(10) #3 | 67.5(3) |
Symmetrical code:
#1x ,-y-1/2 ,-z+1/2;
#2-x-1/2 ,-y-1/2, z;
#3-x-1/2, y ,-z+1/2;
#4x+1/2 ,-y ,-z+1/2;
#5-x-1/2 ,-y, z+1/2;
#6x+1/2, y, z+1/2;
#7-x ,-y, z;
#8-x, y ,-z+1;
#9x ,-y ,-z+1;
#10-x-1 ,-y, z;
#11-x-1/2 ,-y, z-1/2;
#12x-1/2, y, z-1/2.
Claims (3)
- The preparation method of 1.Ba/Fe/Na metal and carboxylic acid schiff bases complex, is characterized in that comprising the steps:The synthesis of assorted metal complexes: get barium chloride dihydrate 0.12 mmol, ferric chloride hexahydrate 0.03 mmol, sodium-chlor 0.06 mmol and H 4l part 0.03 mmol, puts into 15 mL tetrafluoroethylene reactors, and with 1 mL dimethyl formamide, 4 mL ethanol and 2 mL water are mixed solvent, places in an oven, is heated to 100 DEG C of constant temperature 72 hours, then slowly drops to room temperature and get final product.
- 2., according to title complex prepared by preparation method according to claim 1, it is characterized in that its chemical formula is [BaNa (Fe-L) 2( μ 2 -OH) (H 2o)] DMF2H 2o, its crystal belongs to rhombic system, and spacer is f222, unit cell parameters is a=31.955 (3), b=65.386 (2), c=12.9570 (16), α=90 °, β=90 °, γ=90 °, v=27072 (4) 3, basic structure is the three-dimensional frame structure containing duct.
- 3. according to title complex according to claim 2 as the application of Photodegradation catalyst in material science.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273557A (en) * | 2018-02-09 | 2018-07-13 | 长江水利委员会长江科学院 | A kind of iron schiff bases compound photochemical catalyst and preparation method thereof |
| CN108273557B (en) * | 2018-02-09 | 2019-05-03 | 长江水利委员会长江科学院 | A kind of iron schiff bases compound photochemical catalyst and preparation method thereof |
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